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Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (4)
- 1.4 Prozessanalytik (4)
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- 4 Material und Umwelt (3)
- 4.1 Biologische Materialschädigung und Referenzorganismen (2)
- 5.4 Multimateriale Fertigungsprozesse (2)
- 5.6 Glas (2)
- 6.3 Strukturanalytik (2)
- 6.5 Synthese und Streuverfahren nanostrukturierter Materialien (2)
The CCQM-K148.a comparison was coordinated by the BIPM on behalf of the CCQM Organic Analysis Working Group for NMIs and DIs which provide measurement services in organic analysis under the CIPM MRA. It was undertaken as a "Track A" comparison within the OAWG strategic plan. CCQM-K148.a demonstrates capabilities for assigning the mass fraction content of a solid organic compound having moderate molecular complexity, where the compound has a molar mass in the range (75 - 500) g/mol and is non-polar (pKow < −2), when present as the primary organic component in a neat organic solid and where the mass fraction content of the primary component in the material is in excess of 950 mg/g.
Participants were required to report the mass fraction of Bisphenol A present in one supplied unit of the comparison material. Participants using a mass balance method for the assignment were also required to report their assignments of the impurity components present in the material. Methods used by the seventeen participating NMIs or DIs were predominantly based on either stand-alone mass balance (summation of impurities) or qNMR approaches, or the combination of data obtained using both methods. The results obtained using thermal methods based on freezing-point depression methods were also reported by a limited number of participants. There was excellent agreement between assignments obtained using all three approaches to assign the BPA content.
The assignment of the values for the mass fraction content of BPA consistent with the KCRV was achieved by most of the comparison participants with an associated relative standard uncertainty in the assigned value in the range (0.1 - 0.5)%.
Recent DNA-based studies have shown that the built environment is surprisingly rich in fungi. These indoor fungi – whether transient visitors or more persistent residents – may hold clues to the rising levels of human allergies and other medical and building-related health problems observed globally. The taxo¬nomic identity of these fungi is crucial in such pursuits. Molecular identification of the built mycobiome is no trivial undertaking, however, given the large number of unidentified, misidentified, and technically compromised fungal sequences in public sequence databases. In addition, the sequence metadata required to make informed taxonomic decisions – such as country and host/substrate of collection – are often lacking even from reference and ex-type sequences. Here we report on a taxonomic annotation workshop (April 10–11, 2017) organized at the James Hutton Institute/University of Aberdeen (UK) to facilitate reproducible studies of the built mycobiome. The 32 participants went through public fungal ITS bar¬code sequences related to the built mycobiome for taxonomic and nomenclatural correctness, technical quality, and metadata availability. A total of 19,508 changes – including 4,783 name changes, 14,121 metadata annotations, and the removal of 99 technically compromised sequences – were implemented in the UNITE database for molecular identification of fungi (https://unite.ut.ee/) and shared with a range of other databases and downstream resources. Among the genera that saw the largest number of changes were Penicillium, Talaromyces, Cladosporium, Acremonium, and Alternaria, all of them of significant importance in both culture-based and culture-independent surveys of the built environment.
Size and shape are crucial parameters which have impact on the potential of nanoparticles to penetrate cell membranes and epithelial barriers. Current research in nanotoxicology additionally focuses on particle coating. To distinguish between core- and coating-related effects in nanoparticle uptake and translocation, two nanoparticles equal in size, coating and charge but different in core material were investigated.
Silver and iron oxide nanoparticles coated with poly(acrylic acid) were chosen and extensively characterized by small-angle x-ray scattering, nanoparticle tracing analysis and transmission electron microscopy (TEM). Uptake and transport were studied in the intestinal Caco-2 model in a Transwell System with subsequent elemental analysis. TEM and ion beam microscopy were conducted for particle visualization.
Although equal in size, charge and coating, the behavior of the two particles in Caco-2 cells was different: while the internalized amount was comparable, only iron oxide nanoparticles additionally passed the epithelium. Our findings suggest that the coating material influenced only the uptake of the nanoparticles whereas the translocation was determined by the core material.
Knowledge about the different roles of the particle coating and core materials in crossing biological barriers will facilitate toxicological risk assessment of nanoparticles and contribute to the optimization of pharmacokinetic properties of nano-scaled pharmaceuticals.
For the assessment of the barrier function of the geosphere around a nuclear waste repository information about the nature of the accessible rock pore space and internal surfaces is needed. Intact samples of various types of fresh and altered crystalline rocks have been studied by means of mercury intrusion porosimetry and gas adsorption methods using various adsorbates. Furthermore, fluorescence microscopy and scanning electron microscopy was applied and the results were compared with those of impregnation with carbon-l4-polymethylmethacrylate (PMMA). Additional structural information was derived from hydraulic conductivity determinations using helium gas.
The investigations were focussed on the reliability of these measurements of intact core samples, the influence of rock composition, structure and geological evolution on the microstructure of the matrices and the consequences regarding the retardation properties of the bedrock.
Bundling analytical capacities to understand phase formation in recycling of functional materials
(2019)
Transitioning from combustion engine-driven transportation to e-mobility demands a paradigm shift – from a system geared to maximize energy efficiency (i.e. fuel consumption) to a system that may be constrained by the availability of high technology (critical) metals required for electrical energy storage systems and drives. In the wake of these developments efforts in securing new resources of these metals from recycling of end-of-life products are increasing steadily.
Recycling of Li-Ion batteries has recently been evaluated. The results pinpoint to a critical need for understanding slag Formation and its dependence on metal components like Mn under extreme conditions. This will allow researchers to predict optimal Operation setting and to react quickly to changing market demands (which may be Li or Co at one point but may also shift to Ni or rare earth elements (REE)). The long-term goal is to control the formation of specific phases in slags allowing for a Maximum yield of elements of interest and optimal recovery in the separation processes that follows. The combination of data on the physical micro structure and local chemistry of the multi-Phase products during and after processing will help to understand and derive thermodynamic and kinetic data on its formation.
In this paper we are giving an overview on the analytical challenges and approaches to provide robust data on local element concentration and species (especially Mn which is a common component of next generation Li-ion batteries cathodes), spanning the dimensions from the nanometer scale to the bulk material. The complementary interactions of X-rays and electrons make them ideal probes to collect Interface and “in-depth” information. Before- and -after studies as well as in situ structural changes and Phase (trans)formation, changes in elemental and elemental species (e.g. oxidation state) distribution may be tracked by X-ray diffraction (XRD), X-ray fluorescence microscopy and X-ray Absorption spectroscopy. The application of such advanced analytical tools will not only provide essential clues during early lab-based experiments towards the development of new recycling technologies, but may also be deployed for on-line and in-line monitoring of industrial processes.
Aluminum has gathered toxicological Attention based on relevant human exposure and its suspected hazardous potential. Nanoparticles from food supplements or Food contact materials may reach the human gastrointestinal tract.
Here, we monitored the physicochemical fate of aluminum containing nanoparticles and aluminum ions when passaging an in vitro model of the human gastrointestinal tract. Smallangle X-ray scattering (SAXS), transmission electron microscopy (TEM), ion beam microscopy (IBM), secondary ion beam mass spectrometry (TOF-SIMS), and inductively coupled plasma mass spectrometry (ICP-MS) in the singleparticle mode were employed to characterize two aluminumcontaining nanomaterials with different particle core materials (Al0, γAl2O3) and soluble AlCl3. Particle size and shape remained unchanged in saliva, whereas strong Agglomeration of both aluminum nanoparticle species was observed at low pH in gastric fluid together with an increased ion release. The levels of free aluminum ions decreased in intestinal fluid and the particles deagglomerated, thus liberating primary particles again. Dissolution of nanoparticles was limited and substantial changes of their shape and size were not detected. The amounts of particle-associated phosphorus, chlorine, potassium, and calcium increased in intestinal fluid, as compared to nanoparticles in standard dispersion.
Interestingly, nanoparticles were found in the intestinal fluid after addition of ionic aluminum. We provide a comprehensive characterization of the fate of aluminum nanoparticles in simulated gastrointestinal fluids, demonstrating that orally ingested nanoparticles probably reach the intestinal epithelium. The balance between dissolution and de novo complex formation should be considered when evaluating nanotoxicological experiments.
The application of appropriate analytical techniques is essential for nanomaterial (NM) characterization. In this study, we compared different analytical techniques for NM analysis. Regarding possible adverse health effects, ionic and particulate NM effects have to be taken into account. As NMs behave quite differently in physiological media, special attention was paid to techniques which are able to determine the biosolubility and complexation behavior of NMs. Representative NMs of similar size were selected: aluminum (Al0) and aluminum oxide (Al2O3), to compare the behavior of metal and metal oxides. In addition, titanium dioxide (TiO2) was investigated. Characterization techniques such as dynamic light scattering (DLS) and nanoparticle tracking analysis (NTA) were evaluated with respect to their suitability for fast characterization of nanoparticle dispersions regarding a particle's hydrodynamic diameter and size distribution. By application of inductively coupled plasma mass spectrometry in the single particle mode (SP-ICP-MS), individual nanoparticles were quantified and characterized regarding their size. SP-ICP-MS measurements were correlated with the information gained using other characterization techniques, i.e. transmission electron microscopy (TEM) and small angle X-ray scattering (SAXS). The particle surface as an important descriptor of NMs was analyzed by X-ray diffraction (XRD). NM impurities and their co-localization with biomolecules were determined by ion beam microscopy (IBM) and confocal Raman microscopy (CRM). We conclude advantages and disadvantages of the different techniques applied and suggest options for their complementation. Thus, this paper may serve as a practical guide to particle characterization techniques.
Uptake and molecular impact of aluminum-containing nanomaterials on human intestinal caco-2 cells
(2018)
Aluminum (Al) is one of the most common elements in the earth crust and increasingly used in food, consumer products and packaging. Its hazard potential for humans is still not completely understood. Besides the metallic form, Al also exists as mineral, including the insoluble oxide, and in soluble ionic forms. Representatives of these three species, namely a metallic and an oxidic species of Al-containing nanoparticles and soluble aluminum chloride, were applied to human intestinal cell lines as models for the intestinal barrier. We characterized physicochemical particle parameters, protein corona composition, ion release and cellular uptake. Different in vitro assays were performed to determine potential effects and molecular modes of Action related to the individual chemical species. For a deeper insight into signaling processes, microarray transcriptome analyses followed by bioinformatic data analysis were employed. The particulate Al species showed different solubility in biological media. Metallic Al nanoparticles released more ions than Al2O3 nanoparticles, while AlCl3 showed a mixture of dissolved and agglomerated particulate entities in biological media. The protein corona composition differed between both nanoparticle species. Cellular uptake, investigated in transwell experiments, occurred predominantly in particulate form, whereas ionic Al was not taken up by intestinal cell lines. Transcellular transport was not observed. None of the Al species showed cytotoxic effects up to 200 mg Al/mL. The transcriptome analysis indicated mainly effects on oxidative stress pathways, xenobiotic metabolism and metal homeostasis. We have shown for the first time that intestinal cellular uptake of Al occurs preferably in the particle form, while toxicological effects appear to be ion-related.
Microorganisms accumulate molar concentrations of compatible solutes like ectoine to prevent proteins from denaturation. Direct structural or spectroscopic information on the mechanism and about the hydration shell around ectoine are scarce. We combined surface plasmon resonance (SPR), confocal Raman spectroscopy, molecular dynamics simulations, and density functional theory (DFT) calculations to study the local hydration shell around ectoine and its influence on the binding of a gene-S-protein (G5P) to a single-stranded DNA (dT(25)). Due to the very high hygroscopicity of ectoine, it was possible to analyze the highly stable hydration shell by confocal Raman spectroscopy. Corresponding molecular dynamics simulation results revealed a significant change of the water dielectric constant in the presence of a high molar ectoine concentration as compared to pure water. The SPR data showed that the amount of protein bound to DNA decreases in the presence of ectoine, and hence, the protein-DNA dissociation constant increases in a concentration-dependent manner. Concomitantly, the Raman spectra in terms of the amide I region revealed large changes in the protein secondary structure. Our results indicate that ectoine strongly affects the molecular recognition between the protein and the oligonudeotide, which has important consequences for osmotic regulation mechanisms.
The use of biodegradable bone substitutes is advantageous for alveolar ridge augmentation because it avoids second-site surgery for autograft harvesting. This study examines the effect of novel, rapidly resorbable calcium phosphates and a calcium phosphate bone cement on the expression of bone-related genes and proteins by human bone-derived cells (HBDCs) and compares this behavior to that of tricalciumphosphate (TCP). Test materials were -TCP, two materials with a crystalline phase Ca2KNa(PO4)2 and with a small amorphous portion containing either magnesium potassium phosphate (material denominated GB14) or silica phosphate (material denominated GB9), and a calcium phosphate bone cement (material denominated Biocement D). HBDCs were grown on the substrata for 3, 7, 14, and 21 days, counted, and probed for various mRNAs and proteins (type I collagen, osteocalcin, osteopontin, osteonectin, alkaline phosphatase, and bone sialoprotein). All substrates supported continuous cellular growth for 21 days. In the presence of GB14 and Biocement D specimens cell proliferation was reduced and cell differentiation increased. At day 21, the greatest number of cells was found on GB9 expressing significantly higher levels of bone-related proteins than cells grown on all other surfaces. Because all novel materials facilitated the expression of the osteoblastic phenotype at least as much as TCP and the polystyrene control, these biomaterials can be regarded as excellent candidate bone substitute materials. GB9 induced the highest proliferation and cellular differentiation after 21 days of incubation, suggesting that this material may possess a higher potency for enhancing osteogenesis than TCP. © 2004 Wiley Periodicals, Inc. J Biomed Mater Res 69A: 145-154, 2004
X-ray computed tomography (CT) and mercury porosimetry were combined to connect density gradients and the distribution of open porosity in a sintered compact. CT clearly showed that open porosity follows the initial distribution of low-density zones. Mercury porosimetry detected three distinct levels of porosity. Microstructural examination correlated the porosity level with the coordination of (i) two to three or (ii) multiple grains around pores. This combination of techniques provides a novel tool for the study of pore and density-gradient evolution during sintering.
Nanofibers are drawing the attention of engineers and scientists because their large surface-to-volume ratio is favorable for applications in medicine, filter technology, textile industry, lithium-air batteries, and optical sensors. However, when transferring nanofibers to a technical product in the form of a random network of fibers, referred to as nonwoven fabric, the stickiness of the freshly produced and thus fragile nanofiber nonwoven remains a problem. This is mainly because nanofibers strongly adhere to any surface because of van der Waals forces. In nature, there are animals that are actually able to efficiently produce, process, and handle nanofibers, namely cribellate spiders. For that, the spiders use the calamistrum, a comb-like structure of modified setae on the metatarsus of the hindmost (fourth) legs, to which the 10–30 nm thick silk nanofibers do not stick due to a special fingerprint-like surface nanostructure. In this work, we present a theoretical model of the interaction of linear nanofibers with a sinusoidally corrugated surface. This model allows for a prediction of the adhesive interaction and, thus, the design of a suitable surface structure to prevent sticking of an artificially nonwoven of nanofibers. According to the theoretical prediction, a technical analogon of the nanoripples was produced by ultrashort pulse laser processing on different technically relevant metal surfaces in the form of so-called laser-induced periodic surface structures (LIPSS). Subsequently, by means of a newly established peel-off test, the adhesion of an electrospun polyamide fiber-based nonwoven was quantified on such LIPSS-covered aluminium alloy, steel, and titanium alloy samples, as well as on polished (flat) control samples as reference and, additionally, on samples with randomly rough surfaces. The latter revealed that the adhesion of electrospun nanofiber nonwoven is significantly lowered on the nanostructured surfaces compared with the polished surfaces.
The Global Exploration Strategy of the International Space Exploration Coordination Group (ISECG) describes a timeframe of 2020 and beyond with the ultimate aim to establish a human presence on Mars towards the 2040ies. The next steps lie on the Moon with a focus on the coming 10 years. Early lunar surface missions will establish a capability in support of lunar science and prepare and test mission operations for subsequent human exploration of Mars and long-duration human activities on the Moon.
Given the extreme costs involved in the shipping of material from Earth, a prerequisite for future human exploration is the manufacturing of elements directly on the Moon’s surface. Unlike the equipment, which at the beginning will have to be brought from Earth, raw materials and energy could be available following the concept of In-Situ Resource Utilization. The ESA OSIP PAVING THE ROAD (PAVER) study investigates the use of a laser to sinter regolith into paving elements for use as roadways and launch pads thus mitigating dust issues for transport and exploration vehicles.
The ESA-funded study examines the potential of using a laser (12 kW CO2 laser with spot beam up to 100 mm) for layer sintering of lunar and martian regolith powders to manufacture larger 3D elements and provide know-how for the automatic manufacture of paving elements in the lunar environment. The project contributes to the first step toward the establishment of a lunar base and will lead to the construction of equipment capable of paving areas and manufacturing 3D structures.
PAVER project sets the starting point for an examination of the larger context of lunar exploration. Mission scenarios will look at different phases of lunar exploration: Robotic Lunar Exploration, Survivability, Sustainability, and Operational Phase. A proposed Technology Roadmap investigates the mission scenario and analyses how, and to which extent, laser melting/sintering will play a role in the various phases of exploration. The paper contextualizes laser sintering within selected mission scenarios and discusses the different kinds of infrastructure that can be produced at each phase of the mission. The outcome of the study includes the detailing of the TRL steps in the project and an outline of a timeline for the different elements. Covered aspects include terrain modelling such as operation pads, roadways, or towers, non-pressurized building structures to protect machinery, and habitat envelopes, to protect and shield humans against dust, micrometeoroids, and radiation.
Instead of foreseeing and preparing for all possible scenarios of machine failures, accidents, and other challenges arising in space missions, it appears logical to take advantage of the flexibility of additive manufacturing for “in-space manufacturing” (ISM). Manned missions into space rely on complicated equipment, and their safe operation is a great challenge. Bearing in mind the absolute distance for manned missions to the Moon and Mars, the supply of spare parts for the repair and replacement of lost equipment via shipment from Earth would require too much time. With the high flexibility in design and the ability to manufacture ready-to-use components directly from a computer-aided model, additive manufacturing technologies appear to be extremely attractive in this context. Moreover, appropriate technologies are required for the manufacture of building habitats for extended stays of astronauts on the Moon and Mars, as well as material/feedstock. The capacities for sending equipment and material into space are not only very limited and costly, but also raise concerns regarding environmental issues on Earth. Accordingly, not all materials can be sent from Earth, and strategies for the use of in-situ resources, i.e., in-situ resource utilization (ISRU), are being
envisioned. For the manufacturing of both complex parts and equipment, as well as for large infrastructure, appropriate technologies for material processing in space need to be developed.
Die Anwendung von modernen Lehmbaustoffen hat in den letzten Jahren überdurchschnittliche Wachstumsraten erreicht. Für Bauherren und Planer ausschlaggebend ist häufig ihr extrem niedriger CO2-Äquivalentkennwert. Entsprechend wurden Lehmplatten in einem Projekt mit Pilotcharakter für den Umbau des alten Abgeordnetenhauses in Bonn zum Gebäude des Klimareferats der Vereinten Nationen verwendet. Bei der Entscheidung für die Bauweise mit Lehmplatten standen vor allem raumklimatische und schallschutztechnische, das heißt gesundheitliche Aspekte, aber auch der Wunsch nach erhöhter Nachhaltigkeit im Vordergrund. Durch das Fehlen einer Norm entstehen im Vergleich zu geregelten Bauprodukten jedoch noch deutliche Wettbewerbsnachteile für Produzenten von Lehmplatten. Planer und Anwender sehen aufgrund fehlender Prüfzertifikate nicht selten von der Anwendung dieser Lehmbaustoffe ab. Wie schon für Lehmsteine und Lehmmörtel sollen deshalb jetzt auch für Lehmplatten an der Bundesanstalt für Materialforschung und -prüfung (BAM) in dem Projekt StandardBoard Grundlagen für eine Produktnorm geschaffen werden. Darin ist als Projektpartner der Hersteller Conluto beteiligt. Zweck des in Erarbeitung befindlichen Regelwerks ist es, über die Festlegung von Qualitätsanforderungen und Prüfvorschriften die Gebrauchstauglichkeit von Lehmplatten sicherzustellen und somit einerseits Sicherheit für Planer und Anwender und andererseits Vergleichbarkeit und damit Konkurrenzfähigkeit zu konventionellen Plattenprodukten für gleiche Einbaubereiche zu erreichen. Darüber hinaus stellt sie ein Instrument dar, um die besonderen ökologischen und bauphysikalischen Eigenschaften der Lehmbaustoffe hervorzuheben. Die Erarbeitung des Regelwerks erfolgt in enger Abstimmung mit dem Dachverband Lehm e. V. (DVL).
What Does Ectoine Do to DNA? A Molecular-Scale Picture of Compatible Solute−Biopolymer Interactions
(2020)
Compatible solutes are accumulated in the cytoplasm of halophilic microorganisms. These molecules enable their survival in a high salinity environment. Ectoine is such a compatible solute. It is a zwitterionic molecule which strongly interacts with surrounding water molecules and changes the dynamics of the local hydration shell. Ectoine interacts with biomolecules such as lipids, proteins and DNA. The molecular interaction between ectoine and biomolecules in particular the interaction between ectoine and DNA is far from being understood.
In this paper we describe molecular aspects of the interaction between ectoine and double stranded DNA(dsDNA). Two 20 base pairs long dsDNA fragments were immobilized on a Gold surface via a thiol-tether. The interaction between the dsDNA monolayers with diluted and concentrated ectoine solutions was examined by means of X-ray photoelectron and polarization modulation infrared reflection absorption spectroscopies (PM IRRAS). Experimental results indicate that the ability of ectoine to bind water reduces the strength of hydrogen bonds formed to the ribose-phosphate backbone in the dsDNA. In diluted (0.1 M) ectoine solution, DNA interacts predominantly with water molecules. The sugar-phosphate backbone is involved in the formation of strong hydrogen bonds to water, which with elapsing time leads to a reorientation of the planes of nucleic acid bases. This reorientation destabilizes the hydrogen bonds strength between the bases and leads to a partial dehybridizaiton of the dsDNA. In concentrated ectoine solution (2.5 M), almost all water molecules interact with ectoine. Under this condition ectoine is able to interact directly with DNA. Density functional theory (DFT) calculations demonstrate that the direct interaction involves the nitrogen atoms in ectoine and phosphate groups in the DNA molecule. The results of the quantum chemical calculations Show that rearrangements in the ribose-phosphate backbone, caused by a direct interaction with ectoine, facilitates contacts between O atom in the phosphate group and H atoms in a nucleic acid base. In the PM IRRA spectra, an increase in the number of the IR absorption modes in the base pair frequency region proves that the hydrogen bonds between bases become weaker.
Thus, a sequence of reorientations caused by interaction with ectoine leads to a breakdown of hydrogen bonds between bases in the double helix.
Accelerator magnets that can reach magnetic fields well beyond the Nb-Ti performance limits are presently being built and developed, using Nb3Sn superconductors. This technology requires reaction heat treatment (RHT) of the magnet coils, during which Nb3Sn is formed from its ductile precursor materials (a “wind and react” approach). The Nb3Sn microstructure and microchemistry are strongly influenced by the conductor fabrication route, and by the Phase changes during RHT. By combining in situ differential scanning calorimetry, high Energy synchrotron x-ray diffraction, and micro-tomography experiments, we have acquired a unique data set that describes in great detail the phase and microstructure changes that take place during the processing of restacked rod process (RRP), powder-in-tube (PIT), and internal tin (IT) Nb3Sn wires. At temperatures below 450 ° the phase evolutions in the three wire types are similar, with respectively solid state interdiffusion of Cu and Sn, Cu6Sn5 formation, and Cu6Sn5 peritectic transformation. Distinct differences in phase evolutions in the wires are found when temperatures exceed 450 °C. The volume changes of the conductor during RHT are a difficulty in the production of Nb3Sn accelerator magnets. We compare the wire diameter changes measured in situ by dilatometry with the phase and void volume evolution of the three types of Nb3Sn wire. Unlike the Nb3Sn wire length changes, the wire diameter evolution is characteristic for each Nb3Sn wire type. The strongest volume increase, of about 5%, is observed in the RRP wire, where the main diameter increase occurs above 600 °C upon Nb3Sn formation.